CN107603210A - A kind of flame-retardant polyamide composition and its preparation method and application - Google Patents
A kind of flame-retardant polyamide composition and its preparation method and application Download PDFInfo
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- CN107603210A CN107603210A CN201710864664.6A CN201710864664A CN107603210A CN 107603210 A CN107603210 A CN 107603210A CN 201710864664 A CN201710864664 A CN 201710864664A CN 107603210 A CN107603210 A CN 107603210A
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Abstract
The invention belongs to technical field of polymer materials, more particularly to bromine system flame-retardant polyamide composition, and in particular to a kind of high heat-resistant with highly effective flame-retardant, high CTI value and high glow-wire GWIT values separates out bromine system flame-retardant polyamide composition of fastness and its preparation method and application.Flame-retardant polyamide composition provided by the invention, by weight percentage, including component：Polyamide 30~80%；Bromide fire retardant 5~30%；Fire retarding synergist 1~15%；Reinforcing material 0~50%；The fire retarding synergist is stannate and kaolinic composition, and both part by weight are 5:1~1:5.Flame-retardant polyamide composition provided by the invention is while manufacturing cost is reduced, ensure that has excellent flame retardant effect by polyamide material (flame retardant rating is the V0 levels of UL 94, GWIT >=875 DEG C), improving the high temperature resistant processing characteristics of material, injection molding temperature is up to 280 DEG C, or even at 325 DEG C, moulding surface is substantially without precipitation, it is non-discolouring, and there is excellent mechanical property, anti-precipitation performance in wet condition is also preferable.
Description
Technical field
The invention belongs to technical field of polymer materials, more particularly to bromine system flame-retardant polyamide composition, and in particular to one
Kind separates out the inexpensive fire-retardant polyamides of bromine system of fastness with highly effective flame-retardant, high CTI value, high glow-wire GWIT values and high heat-resistant
Amine composition and its preparation method and application.
Background technology
Polyamide has excellent mechanical strength and moulding processability, is able to extensively in fields such as automobile, electronic apparatus
Using.But because burning easily occurs in use for electric equipment products and cause fire, therefore, iing is required that material has
While preferable mechanical property, also require that material has good fire resistance.
The fire retardant species flame-retardant modified available for polyamide mainly has bromine system, phosphorus system, nitrogen system etc..Bromine system fire retardant at present
Be because of its efficiency high, dosage it is few, small and moderate to the performance impact of material, its efficiency/price is than other non-flame-retardant systems
It can be equal to, thus be widely applied, but be usually used in the flame-retardant modified bromide fire retardant of polyamide, such as decabrominated dipheny second
Alkane, brominated Polystyrene (BPS), brominated polystyrene (PBS) etc., it can all contain a certain amount of free bromine, at least typically 10ppm
Left and right, at most 30-50ppm, cause bromine system fire-retardant polyamide material can be by with the extension of heated time in injection molding process
Free bromine and bromination hydrogen are gradually discharged, and inductive effect be present, causes article surface easily to change colour jaundice even blackening, especially
When being the big product of higher temperature (more than 280 DEG C) injection molding light color or small complex thin wall parts, because cycle period is longer, become
Pornographic condition is even more serious, can not meet the requirement of engineering equipment or electronic electric equipment, especially household electrical appliance working of plastics.
In addition, in injection molding process, fire retardant can also decompose generation small-molecule substance, adsorb in mould or article surface, therefore be molded
The precipitate on frequently cleaning mold surface is needed during processing, it is difficult to realize continuous production, cause production and processing efficiency low, therefore solve
Certainly discoloration of the bromine system fire-retardant polyamide material in injection molding process, precipitation problem are significant.
Furthermore to reach more preferable flame retardant effect, the bromide fire retardant fire retarding synergist that would generally arrange in pairs or groups is used together, at present
The most frequently used fire retarding synergist is antimony oxide.Ministry of Land and Resources's issue control antimony ore exploitation total amount requirement in 2011, antimony money
Source is lasting in short supply, causes antimony oxide price constantly to be ascended to heaven, and finds antimony oxide substitute and has brought into schedule.And use
Antimony oxide is relatively low as the phase ratio creepage tracking index (CTI) of fire retarding synergist, will be typically less than 300V, and injection molding
When can produce a large amount of gases, be more easy to make moulding change colour.
The fire retarding synergist that can partly substitute antimony oxide developed in recent years has Firebrake ZB, zinc sulphide, zirconium chemical combination
Thing and molybdenum compound, although these substitutes have played good fire-retardant synergistic effect in some flame retardant plastics, on the one hand
These substitutes are expensive, on the other hand can only also substitute 30% or so antimony, while also to increase the dosage of synergistic combustion adjuvant,
It is relatively low to consequently leads to its comprehensive mechanical property.
The A of Chinese patent CN 102604377 disclose a kind of flame-proofed thermoplastic daiamid composition, its component and weight hundred
Fraction composition is as follows：(1) thermoplastic polyamide resin 30-90%；(2) bromide fire retardant 5-40%；(3) fire retarding synergist 0.5-
15%；(4) reinforcing material 0-50%.The patent application is by the way that brominated Polystyrene, Firebrake ZB, organic silicon fibre retardant are compounded
To a kind of flame-proofed thermoplastic daiamid composition, antimonial is instead of with organic silicon fibre retardant, reduces bromine to a certain extent
Antimony synergy caused by a large amount of gases, meet environmental protection requirement, but in the market some common are machine silicon fire retardant valency
Lattice are all universal higher, and this causes the cost of the system to uprise.Furthermore Firebrake ZB is as fire retarding synergist, Flameproof polyamide product
Deposited for a long time or in wet environment using that there can be boric acid precipitation, so as to influence outward appearance and electrical property.
The A of Chinese patent CN 102604375 disclose a kind of inexpensive high fire-retardance reinforced polyamide and preparation method thereof, should
Using bromide fire retardant as main flame retardant, fire retarding synergist is that stannate composite flame-retardant agent and ultra-fine Magnesiosilicates synergistic hinder for invention
The compound of agent is fired, obtained fire-retarding reinforced polyamide has high intensity, fire-retardant to meet UL94V0 levels.But current commodity is super
Thin Magnesosilicate has the following disadvantages：Heatproof is low, is easily separated out in injection molding process, the combination of obtained fire-retarding reinforced polyamide
Thing mechanical property, electrical property (CTI value 350V) and glowing filament ignition temperature (850 DEG C of GWIT values) be not high.
The content of the invention
It is an object of the present invention in view of the shortcomings of the prior art, production is a kind of to have highly effective flame-retardant, high CTI value, Gao Zhuo
Heated filament GWIT values, high heat-resistant separate out the inexpensive bromine system flame-retardant polyamide composition of fastness.To achieve the above object, this hair
It is bright to adopt the following technical scheme that：
A kind of flame-retardant polyamide composition, by weight percentage, including following component：
The fire retarding synergist is stannate and kaolinic composition, and both part by weight are 5:1~1:5.Compare
In antimony oxide, the compatibility and bonding force of stannate and polyamide are very good, and dispersiveness is good in polyamide, and kaolin
Compounding use, the two gives full play to synergistic function, can 100% substitution antimony oxide completely, by regulate and control stannate with
Kaolinic dosage, the CTI values and glowing filament GWIT of polyamide material can be effectively improved while reaching excellent flame retardant effect
Value.
Preferably, described flame-retardant polyamide composition, by weight percentage, including following component：
Preferably, when the stannate in flame retarded wall and kaolinic weight ratio are 3:4~2:When in the range of 1, two
Person can play more preferable cooperative effect, and with the proportion increase of stannate, the combination property of composition is more preferably.
Wherein, the polyamide is selected from PA6, PA66, PA46, PA66/6, PA610, PA611, PA612, PA6T/
66th, at least one of PA9T.
Wherein, the bromide fire retardant is selected from TDE, brominated Polystyrene, brominated polystyrene, poly- pentabromo-
At least one of benzyl acrylic ester, bromination polyphenylene ether.
Wherein, the stannate is selected from zinc stannate, zinc hydroxyl stannate, calcium stannate, magnesium stannate, cobaltous stannate, sodium stannate, stannic acid
At least one of potassium, stannic acid silicon.
Wherein, the kaolin is composition using alumino-silicate as main component, including water-washed kaoline, calcining kaolinite
Soil.The kaolin can be kaolin inorganic or by the coupling agent treatment such as amino silane, this kind of idol
Join agent such as DOW31-441, TEGOMER V-Si4042.The kaolin treated through amino silicane coupling agent
More preferable compatibility is shown with polyamide, makes the mechanical property of polyamide modified material more excellent.
The reinforcing material is selected from E glass fibres, B glass fibres, carbon fiber, aromatic polyamide fibre, wollastonite fibre, pottery
Porcelain fiber, potassium titanate crystal whisker, alkali magnesium sulfate crystal whisker, silicon carbide whisker or silica, alumina silicate, silica, titanium dioxide,
The powderies such as talcum, wollastonite, diatomite, clay, kaolin, globular glass, mica, gypsum, iron oxide, magnesia and zinc oxide
Or at least one of inorganic compound of tabular.
The composition of the present invention can add other components according to being actually needed, and other components include lubricant, toughness reinforcing
In agent, impact modifying agent, releasing agent, heat stabilizer, light stabilizer, antistatic additive, ultraviolet absorber, colouring agent and antioxidant
It is one or more of.
The preparation method of above-mentioned flame-retardant polyamide composition, including step：Produced, utilized using melt blending expressing technique
Single screw extrusion machine, double screw extruder or multi-screw extruder, add polyamide from main spout, partly or entirely increase
Strong material, fire retardant and fire retarding synergist, side spout add remaining reinforcing material；After melt blending, through cooling down, air-dry and
It is granulated.
Flame-retardant polyamide composition provided by the invention can be by extruding, being molded or compression molding is product, for low
Voltage breaker housing, coil rack, car electrics, industrial electrical equipment housing, A.C. contactor shell and electronic connector etc. zero
Part.
Compared with prior art, the present invention has the advantage that as follows：
1) it is of the invention using the stannate (1% thermal weight loss temperature >=340 DEG C) with excellent heat resistance and kaolinic
Composition ensure that polyamide material has excellent flame retardant effect (fire-retardant as the fire retarding synergist in bromine system flame-retardant system
Grade is UL94V0 levels, GWIT >=875 DEG C), the high temperature resistant processing characteristics of material is improved, injection molding temperature is up to 280 DEG C,
Even 325 DEG C, substantially without precipitation in injection moulding process, moulding is also basically unchanged color, while has excellent mechanical property, in tide
Anti- precipitation performance under wet environment is also preferable, and safety is provided for use of the Flameproof polyamide product on high request electronic apparatus
Ensure.
2) flame retarded wall of the invention can substitute the exotic material antimony oxide of the exploitation of country's limitation at present, reach
The preferential strategic resource of the rare antimony resource country of saving and the purpose for reducing production cost, compared to bromine/antimony system Flameproof polyamide
System, the surface insulation performance of fire-retardant polyamide material of the invention are improved, and CTI values >=475V, are enhanced in use
Security performance and electric property.
Embodiment
With reference to embodiment, the invention will be further described：
It is that the present invention will be further described for embodiment with lower part, but implementation below is only to this hair
Bright is explained further, and does not represent the scope of the present invention and is only limitted to this, the equivalence replacement that every thinking with the present invention is done,
In protection scope of the present invention.
PA6：M2400, Meida Nylon Co., Ltd., Xinhui, Guangdong；
PA66：EPR27, China Shenma Group Co., Ltd.；
Glass：ECS301CL-4.5, Chongqing Polycomp International Co., Ltd；
TDE：Shandong Haiwang Chemical Co., Ltd.；
Antimony oxide：GuangXi HuaTi Science Co., Ltd；
Brominated Polystyrene (BPS)：Shandong Tianyi Chemical Co., Ltd.；
Brominated polystyrene (PBS)：Shandong Tianyi Chemical Co., Ltd.；
Firebrake ZB：Shandong Chuanjun Chemical Co., Ltd.；
Magnesium silicate：Prosperous Science and Technology Ltd. is combined in LHX-999, Shenzhen；
Zinc stannate：Shang Haijia wins Trade Co., Ltd.；
Magnesium stannate：Shandong Jiqing Chemical Co., Ltd.；
Stannic acid silicon：Poly- thousand Chemical Co., Ltd. in Shanghai；
Kaolin：China Kaolin Clay Co., Ltd.；
Processing aid：Including lubricant and antioxidant.Lubricant：PETS, send out base chemicals (Zhangjiagang) Co., Ltd；It is anti-
Oxygen agent：Irganox-1098, BASF；Irgafos-168, BASF.
[1~embodiment of embodiment 14]：According to material proportion in table 1 by polyamide, bromide fire retardant, fire-retardant synergistic
After agent and other components add mixer mixing, extruder is added from main spout；Reinforcing material is added by side spout and extruded
Machine.After melt blending, through cooling down, air-drying and be granulated, the performance test results are shown in Table 1.
[1~reference examples of reference examples 14]：Fire retarding synergist is substituted by Firebrake ZB, antimony oxide or ultra-fine magnesium silicate
Salt, each material component proportioning are shown in Table 2, and its preparation method is same with embodiment to be carried out, and obtains being granulated particle, the performance test results are shown in
Table 2.
The following property that sample is made is tested according to following methods：
1st, glowing filament GWIT：60 × 60 × 0.75mm square plates are made by injection moulding, according to GB/T 5169.12-2006
Standard is tested.
2nd, phase ratio creepage tracking index CTI：Diameter 100mm, thickness 3mm disks, according to GB/T are made by injection moulding
4207-2003 standards are tested.
3rd, anti-flammability：125 × 13 × 0.8mm is made by injection moulding, tested according to UL-94 standards.
4th, mechanical property：GB proof forces are made by injection moulding to imitate bar, tensile strength (GB/ is carried out according to national standard
T1040-2006), bending strength (GB/T9341-2000), impact strength (GB/T1843-2008) performance test.
5th, injection stops discoloration：5 mould colour tables and the colour table contrastive colours being routinely molded are injection moulded by stopping 5min
Difference obtains.
6th, it is molded precipitation situation：By being injection moulded 200 mould colour tables, the white precipitation of mould and the precipitation of colour table surface is observed
Material.
7th, wet environment separates out：By the way that colour table is placed 14 days under 50 DEG C, 85%RH environment, observation colour table surface whether there is
White separates out material.
1 embodiment of table, 1~14 each recipe ingredient and the performance test results
Remarks：It is basically unchanged color：Color matching personnel naked eyes can not tell aberration；Pole light discolouration：Only professional color matching personnel
Visually it is distinguishable go out aberration；Light discolouration：Ordinary person carefully recognize it is distinguishable go out aberration；Obvious discoloration：Ordinary person's naked eyes
Aberration can directly be found out.
2 comparative example of table, 1~14 each recipe ingredient and the performance test results
Remarks：It is basically unchanged color：Color matching personnel naked eyes can not tell aberration；Pole light discolouration：Only professional color matching personnel
Visually it is distinguishable go out aberration；Light discolouration：Ordinary person carefully recognize it is distinguishable go out aberration；Obvious discoloration：Ordinary person's naked eyes
Aberration can directly be found out.
Find out, bromine system produced by the present invention flame-retardant polyamide composition that there is excellent flame retardant effect by table 1~2, it is fire-retardant
Grade reaches 1.6mm UL-94V0 levels, even up to 0.8mm UL-94V0 levels, glowing filament ignition temperature GWIT values up to 850~
900 DEG C, CTI values are up to 475~550V, hence it is evident that better than bromine/antimony system Flameproof polyamide (800 DEG C of GWIT values, CTI values 200~
350V)；And high temperature resistance injection molding separates out and discoloration is more excellent.Meanwhile bromine system produced by the present invention Flameproof polyamide
The combination property of material composition, it is only stannate that especially anti-injection molding, which separates out and is substantially better than fire retarding synergist with discoloration,
Or stannate and the performance of other synergist compounding uses；Also overcome the Firebrake ZB synergistic of more common replacement antimony oxide
Precipitation problem when the polyamide material of flame-retardant system uses under long-term wet environment.
In addition, from embodiment 1~5 and embodiment 8~11 as can be seen that when the stannate and kaolinite in flame retarded wall
The weight ratio of soil is 3:4~2:When in the range of 1, the two can play more preferable cooperative effect, with the proportion increase of stannate, group
More preferably, flame retardant rating can reach 0.8mm UL-94V0 levels to the combination property of compound.
Claims (10)
- A kind of 1. flame-retardant polyamide composition, it is characterised in that by weight percentage, including following component：The fire retarding synergist is stannate and kaolinic composition, and both part by weight are 5:1~1:5.
- 2. flame-retardant polyamide composition according to claim 1, it is characterised in that by weight percentage, including it is as follows Component：
- 3. flame-retardant polyamide composition according to claim 1, it is characterised in that：The polyamide be selected from PA6, At least one of PA66, PA46, PA66/6, PA610, PA611, PA612, PA6T/66, PA9T.
- 4. insulating heat-conductive composite according to claim 1, it is characterised in that：The bromide fire retardant is selected from ten bromines two In vinylbenzene, brominated Polystyrene, brominated polystyrene, poly- phenyl-pentabromide methacrylate, bromination polyphenylene ether at least It is a kind of.
- 5. flame-retardant polyamide composition according to claim 1, it is characterised in that the reinforcing material is selected from E glass fibers Dimension, B glass fibres, carbon fiber, aromatic polyamide fibre, wollastonite fibre, ceramic fibre, potassium titanate crystal whisker, alkali magnesium sulfate are brilliant Palpus, silicon carbide whisker or silica, alumina silicate, silica, titanium dioxide, talcum, wollastonite, diatomite, clay, kaolinite At least one in the powderies such as soil, globular glass, mica, gypsum, iron oxide, magnesia and zinc oxide or the inorganic compound of tabular Kind.
- 6. flame-retardant polyamide composition according to claim 1, it is characterised in that the stannate is selected from zinc stannate, hydroxyl At least one of base zinc stannate, calcium stannate, magnesium stannate, cobaltous stannate, sodium stannate, potassium stannate, stannic acid silicon.
- 7. flame-retardant polyamide composition according to claim 1, it is characterised in that the kaolin be using alumino-silicate as The composition of main component, including water-washed kaoline, calcined kaolin.
- 8. flame-retardant polyamide composition according to claim 1, it is characterised in that the component also includes lubricant, increased In tough dose, impact modifying agent, releasing agent, heat stabilizer, light stabilizer, antistatic additive, ultraviolet absorber, colouring agent and antioxidant One or more.
- 9. a kind of preparation method of any described flame-retardant polyamide composition of claim 1~8, including step：Using melting Blending extrusion technique productions, using single screw extrusion machine, double screw extruder or multi-screw extruder, added from main spout poly- Amide resin, part or all of reinforcing material, fire retardant and fire retarding synergist, side spout add remaining reinforcing material；It is molten After melting blending, cooling, air-dry, be granulated.
- 10. the flame-retardant polyamide composition described in any one of claim 1~8 is for manufacturing low-voltage circuit breaker housing, coil Application in skeleton, car electrics, industrial electrical equipment housing, A.C. contactor shell and electronic connector.
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| CN108948734A (en) * | 2018-05-31 | 2018-12-07 | 徐州腾飞工程塑料有限公司 | A kind of high glowing filament ignition temperature flame-retardant enhancing PA6 composite material and preparation method |
| CN109438977A (en) * | 2018-09-30 | 2019-03-08 | 宁波塑之华塑化有限公司 | A kind of stannate fire-retardant nylon and preparation method thereof |
| CN109679329A (en) * | 2018-12-25 | 2019-04-26 | 浙江普利特新材料有限公司 | A kind of high glow-wire, the fire-retardant enhancing copolymer nylon composite material and preparation method of high CTI |
| CN110157123A (en) * | 2018-02-14 | 2019-08-23 | 日立金属株式会社 | Insulation composition and electric wire |
| CN110606957A (en) * | 2019-08-22 | 2019-12-24 | 安徽建筑大学 | Cobalt and zinc hybrid flaky crossed ZIF flame retardant containing stannate ions and preparation method thereof |
| CN110883975A (en) * | 2019-11-06 | 2020-03-17 | 张家港大塚化学有限公司 | Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material |
| CN111100449A (en) * | 2019-12-03 | 2020-05-05 | 天津金发新材料有限公司 | Polyamide composition and preparation method thereof |
| CN112795183A (en) * | 2020-12-30 | 2021-05-14 | 上海普利特复合材料股份有限公司 | High-strength, low-shrinkage and low-precipitation environment-friendly flame-retardant polyamide composition and preparation method thereof |
| CN113388248A (en) * | 2021-07-21 | 2021-09-14 | 合诚技术股份有限公司 | high-CTI brominated flame-retardant reinforced polyamide composite material and preparation method and application thereof |
| CN114316584A (en) * | 2021-12-24 | 2022-04-12 | 浙江普利特新材料有限公司 | Brominated flame-retardant high-heat-resistance bio-based polyamide composition and preparation method thereof |
| CN114957977A (en) * | 2022-04-08 | 2022-08-30 | 北京理工大学 | Microporous-micronucleus functionalized flame-retardant polyamide resin |
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| CN110157123A (en) * | 2018-02-14 | 2019-08-23 | 日立金属株式会社 | Insulation composition and electric wire |
| CN108948734A (en) * | 2018-05-31 | 2018-12-07 | 徐州腾飞工程塑料有限公司 | A kind of high glowing filament ignition temperature flame-retardant enhancing PA6 composite material and preparation method |
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| CN109679329A (en) * | 2018-12-25 | 2019-04-26 | 浙江普利特新材料有限公司 | A kind of high glow-wire, the fire-retardant enhancing copolymer nylon composite material and preparation method of high CTI |
| CN110606957B (en) * | 2019-08-22 | 2021-05-18 | 安徽建筑大学 | Cobalt and zinc hybrid flaky crossed ZIF flame retardant containing stannate ions and preparation method thereof |
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